Apparatus for treatment of hydrocarbon residues



Sept. 9, 1941.

E. J. HOUDRY APPARATUS FOR TREATMENT OF HYDROCARBON RESIDUES Original Filed Nqv.- 2 7, 1935 IINVENTOR MI E Patented Sept. 9, 1941 APPARATUS FOR TREATMENT OF HYDROCARBON RESIDUES Eugene J. Houdry, Ardmore, Pa., assignor to Houdry Process Corporation, Wilmington, Del., a corporation of Delaware Original application November 2'7, 1935, Serial No. 51,770. Divided and this application January 23, 1939, Serial No. 252,288

5Claims.

This invention relates to apparatus for the processing of residues of hydrocarbon material such as those derived from petroleum, shale oil,

bituminous distillates, etc., and is a division of the invention set forth in my copending application Serial No. 51,770, filed November 2'7, 1935. More particularly, it concerns the removal from such residues of certain components such as ash, coke, tarry and resinous material, asphalt and substances which are readily. changed into clean material in vapor phase. Another object a is to produce, in the cleaning or separating operation, a residuum in desirable soft and dry form, and to avoid the formation of a caked, sticky or other hard-to-remove deposit. Another object is to devise simple and easily operated apparatus for accomplishing the above results. Other objects will be apparent from the detailed description which follows.

The invention involves apparatus for the cleaning up, by a thermal filtering operation, of a heavy hydrocarbon stock comprising or containing residual material and the removal of all components not in vapor phase in the form 01' soft, dry coke. The hydrocarbon charge, heated and partly in vapor phase, is fed into the lower end of the separator in such a manner and at a suitable rate to keep. the contents in a state of agitation and to avoid the formation of a pool of oil. The necessary heat for the separating action is preferably supplied entirely or substantially by the incoming charge and the undesirable components are retained in a state of suspension in the separating or expansion chamber until solids drop or are thrown down passageway for the entering charge.- Two or a more separators are preferably used to permit continuous operation, and, from time to time, the charge is switched from one to another to permit removal of the coky deposit, which is easily effected by a simple scraping and blowing operation.

In order to illustrate the invention, one concrete embodiment thereof is shown in the accompanying drawing, in which: I

Fig. 1 is a side elevational view, somewhat diagrammatic in character, with the separator shown in vertical section;'

Fig. 2 is a plan view of a part of the apparatus shown in Fig. 1;

Fig. 3 is a vertical sectional view on an enlarged scale of one of the separators; and

Fig. 4 is a transverse sectional view substantially on the line 44 of Fig. 3.

As indicated in Figs. 1 and 2, the heavy hydrocarbon charge, preferably mixed withsteam, is sent through a heater 5 of any suitable or desired type, such as a tube still, at a relatively high rate to minimize cracking and then passes, by valved line 6, where additional steam may be added, if desired, from line 1, into the lower end of one or more of a battery of separators 8. Two such separators are shown in Fig. 2, the intention being to operate continuously by sen'ding the charge into one separator while a steaming down and cleaning operation is being performed in the other separator, the separators being arranged to alternate in function. The charge enters the lower reduced end 8a of separator 8, then passes upwardly into an expansion chamber 8b, the bottom walls of which taper toward end to. The charge keeps the contents of chamber 8b in a continuous state of agitation, and continuously, supplies heat thereto. The solids are separated out and deposited upon the bottom wall of expansion chamber 81) where they gradually build up a layer'of coky material while leaving a vertical opening or passage for the entering charge. The components in vapor phase pass out of the top of separator 8 into a valved line 9, and are in clean condition suitable for immediate thermal conversion or catalytic transformation or other treatment to produce desirable finished products of the same or different boiling range, or of entirely different composition. Such additional treating apparatus is diagrammatically indicated at ill in Fig. 1. Each As the mass accumulates, it leaves a hole or separator 8 is run for a desired length of time,

which is determined by the accumulation of the deposit and its nature, and then the stream of charging material is sent into another separator while the first is being cleaned of the deposit.

The cleaning operation consists in sending suitable gaseous purging material, such as steam from line I, into the bottom of the separator for a sumcient period to drive out all volatile hydrocarbons which may be retained absorbed'or adsorbed by the deposit. An alternative means is by vacuum purging. Thereupon a scraper ll, operated by a shaft II, which extends through a stuffing box l3 in the top of each separator,

is lowered and rotated by suitable means such as a crank l4 to break up the deposit. After removal of cap l5 or the opening of a suitable valve at this point,-the loosened deposit is blown out through the restricted end 8a into a suitable receptacle 16 by a gaseous ejecting agent, such as steam admitted at the top of the separator from branched line I. Scraper II is provided with an extension Ila of any desired length, to insure the clearing of the restricted lower end 8a.

Scraper H, as indicated in Fig. 4, may comprise a plurality of blades, and, when not in use, the scraper is raised to the top of the separating chamber, as indicated in Fig. 1. To effect a pendent .of course upon the composition of the complete cleaning of the separator, including the thin layer of deposit which may be left by scraper ll, an oxidizing agent, such as air may be admitted by line I! to burn out the chamber.

The thermal filtering or separating action which takes place in expansion chamber 8b involves a certain amount of viscosity breaking of the charge, and the heat for this action is supplied by the incoming stream of mixed steam and hydrocarbons, which preferably enters restricted end 8a of the separator in the temperature range of 850 to 930 F. To take care of heat losses through the walls of the separator, the same may be kept at a constant temperature of the order of 850 F. by external heating means (not shown) such as an electric heating coil or a jacket for flue gases. If needed or desired, a part of the charge may be burned within chamber 81) to supply heat by admitting a small amount of air through line H.

In a typical operation, the charging material was bottoms of East Texas crude oil. This charge was sent through heater 5 and delivered into the restricted bottom 8a of the separator with 20% by weight of steam at an' average temperature of 890- F. The'wall temperature of chamber 8 was kept at 860 F. The, feed rate in liquid per hour was about three times the volume of separator 8, or 3:1. The charging stock had an A.P. I. gravity of 2 13, viscosity at 130 F. of 287, and a viscosity at 210 F. of 75. In an hours run, the overhead material during the first half hour had a gravity of 23.9, viscosity at 130 F, of 164, and viscosity at 210 F. of 53; while, during the second half hour, the overhead had an A. P. I. gravity of 22.8, a viscosity at 130 F. of 218, and a viscosity at 210 of 59. The overhead was a good clean oil. The deposit left in the separator comprised 2.6% by weight of the charged material and the feed rate. The latter canivary from about 1 /2:1 to about 5:1. The quantity of steam or other gaseous material fed with the charge to assist vaporization and to minimize thermal cracking in the heater or still may run from 2 to 30% by weight. When the charging stock comprises heavier hydrocarbons or a lower bottom cut than that indicated in the example in the preceding paragraph, the coky deposit will be laid down at an increased rate and the length of the run on each individual separator will be correspondingly shortened, but the soft, friable character of the deposit will be retained.

From the above, it will be apparent that the present invention provides convenient and emcient means for converting hydrocarbon bottoms into clean vapor phase material suitable as charge to other treating and converting operations, and that the coke, asphalt, ash and other undesirable materials are recovered in a soft, porous, brittle, and hence readily removable form. Apparently, the form of the deposit is due to the novel method of operation, whereby the charge is sent into the bottom of an expansion chamber atlow velocity,

so that it keeps the contents of the chamber continuously in a state of agitation while imparting heat thereto, so that the components of the charge not in vapor phase when they are sent into the expansion chamber are kept in movement until viscosity breaking takes place, with the release of vapor phase material and the dropping out of the remainder in the form of solid parti-. cles which are deposited and build up a layer on the bottom of .the chamber. The purging or steaming out operation following the run not only removes the volatile hydrocarbons which may be in or retained by the solid deposit, but also dries out the latter so that it is readily blown out after being loosened by the scraper.

Aside from its value as fuel, this final coky residuum, containing as it does most if not all of the ash content of the original crude, is important as a convenient source of recovery of certain valuable substances-known to exist in a state of suspension or otherwise in mineral oils.

.The vanadium content of certain crudes, espe- .tanium, sodium and gold in addition to vanadium charge. When analyzed, it was found to contain have been found in the ashes of Mexican oils.

Crudes obtained in the United States contain iron,

aluminum, vanadium and nickel. Recovery of such substances is readily effected by acid leaching or other chemical treatment of the coky deposit produced by the present invention, or by burning the deposit and utilizing precipitation of the fumes to insure recovery even when the desired substances become volatile.

I claim as my invention:

1. Apparatus adapted for use in trained solids and vapors from a mixture thereof comprising a casing having side walls providing an enlarged upper separating chamber for the mixture with a communicating reduced lower chamber for assisting the separation in the upper chamber, outlet means in the upper chamber for the separated vapors, outlet means in the lower chamber for the separated solids, scraping means for loosening the solids, said means during the separating operation being normally retracted upwardly in the separating chamber and separating enthe laterally extending walls, a shaft having one deposit in the casing and scrape the walls of the comprising a reduced lower end and enlarged upper end, said lower end being adapted to drill through any deposit in the casing and. scrape deposit from the walls of the lower chamber and said upper end being adapted to scrape deposit -from the walls of the upper chamber, a

shaft having one end in the casing secured to said scraping means and one end outwardlya thereof and adapted for rotating and lowering the scraping means.

2. Apparatus adapted for use in separating entrained solids and vapors from a mixture thereof comprising a casinghaving side walls providing an enlarged upper separating chamber for the mixture with a communicating reduced lower chamber for assisting the separation in the upper chamber, and laterally extending walls inter-- connecting said chambers, outlet means in the upper chamber for the separated vapors, outlet means in the lower chamber for the separated solids, scraping means for loosening the solids, said means during the separating operation being normally retracted upwardly in the separating chamber and comprising a reduced lower end and enlarged upper end, said lower end being adapted to drill through any deposit in the casing and scrape the walls of the lower chamber and said upper end being adapted to scrape de-' posit from the walls of the upper chamber and end in the casing secured to said scraping means andone end outwardly thereof and adapted for rotating and lowering the scraping means.

3. Apparatus adapted for use in separating entrained solids and vapors from a mixture thereof comprising a casing having side walls providing an enlarged upper separating chamber for the mixture with a communicating reduced lower chamber for assisting the separation in the upper chamber, and inwardly tapering walls interconnecting said chambers, outlet means in the upper chamber for the separated vapors, outlet means in the lower chamber for the separated solids, scraping .means for loosening the solids, said means during the separating operation being normally retracted upwardly in the separating chamber and comprising a reduced lower end and enlarged upper end having inclined shoulders, said lower end being adapted to drill through any lower chamber and said upper end being adapted to scrape depositfrom the walls from the upper chamber and the inwardly taperingwalls, and

a shaft having one end in the casing secured to said scraping means and one end outwardly rthereof and adapted for rotating and lowering the scraping means.

4. Apparatus adapted for use in separating entrained solids and vapors from a mixture thereof comprising a casing having side walls providing an enlarged upper separating chamber for the mixture with a communicating reduced lower chamber for assisting the separationin the upper chamber, outlet means in the upper chamber for the separated vapors, outlet means in the lower chamber for the separated solids, scraping means for loosening the solids, said means during the separating operation being normally retracted upwardLv in the separating chamber and comprising a reduced lower end and enlarged upper end, said lower end being adapted to drill through any deposit in the casing and scrape the walls of the lower chamber and said upper end being adapted to scrape deposit from the wallsof the upper chamber, a shaft having one end in the casing secured to said scraping means and one end outwardly thereof and adapted for rotating and lowering the scraping means, and means for supplying a. fluid medium to the upper chamber for ejecting the loosened solids from the casing.

5. Apparatus adapted for usein separating entrained solids andvapors from a mixture thereof comprising a casing having side walls providing an enlarged upper separating chamber for the mixture with a communicating reduced vlower chamber, means for admitting fluid to the lower chamber for assisting the separation in the upper chamber, outlet means in the upper chamber for the separated vapors, outlet means 'in the lower chamber for the separated solids, scraping means 'f0r loosening the solids, said means during the separating operation being normally retracted upwardly in the separating chamber and comprising a reduced lower end and enlarged upper end, said lower end being adapted to drill through any deposit in the casing and scrape the walls of the lower chamber and said upper end being adapted to scrape deposit from the walls of the upper chamber, a shaft having one end in the casing secured to said scraping means and one end-outwardly thereof and adapted for. rotating and lowering the scraping means, and means for supply...-

ing a fluid medium to the upper chamber for ejecting the loosened solids from the casing. 1

EUGENE J. noumw. 

